CN109879272B - Method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater - Google Patents
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Abstract
The invention discloses a method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater, and belongs to the technical field of carbon quantum dot preparation. Heating tobacco wastewater to 200-300 ℃ at a constant speed, and heating and reacting for 1-3 h in the temperature range until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A; after the reaction product A is cooled to room temperature, adding a modifier into the reaction product A and uniformly mixing to obtain a mixed solution B; and stirring the mixed solution B for 5-10 min, carrying out ultrasonic treatment for 5-10 min, standing, taking supernatant, carrying out centrifugal treatment, standing again, and taking supernatant to obtain the multicolor fluorescent carbon quantum dots dispersed in the modifier. The method takes the tobacco wastewater as a carbon source, prepares the carbon quantum dots through simple pyrolysis reaction, and disperses the carbon quantum dots by respectively taking ethanol, deionized water, oxalic acid and sodium hydroxide solution as modifiers, so that the fluorescence emission wavelength of the carbon quantum dots can be adjusted from a blue region to a yellow region.
Description
Technical Field
The invention relates to a method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater, belonging to the technical field of carbon quantum dot preparation.
Background
The carbon quantum dots are novel zero-dimensional carbon nano-materials with the size less than 20 nm, have excellent fluorescence characteristics and unique chemical, electronic and optical properties. Compared with the traditional dye molecules and semiconductor quantum dots, the carbon quantum dots have the advantages of high chemical stability, low cytotoxicity, biocompatibility, unique electronic and optical properties, metabolic degradation resistance and the like. Therefore, the carbon quantum dots can be widely applied to various fields such as optoelectronic devices, energy conversion, photocatalysis, sensors, biological imaging, cell marking, drug delivery and the like as high-grade fluorescent materials, have great application potential and wide prospect, are paid attention to by academia and industry, and related research and application also rapidly become a new field which is full of vitality and develops at a high speed.
Because the carbon quantum dots have excellent physical and chemical properties and wide application prospects, more and more preparation methods are developed and adopted. The top-down method mainly comprises photoetching graphite microcrystals by utilizing a high-resolution electron beam, and treating carbon fibers and carbon black by hydrothermal cutting, an electrochemical approach or chemical oxidation, and the methods all require special equipment and special synthesis conditions, and the prepared carbon quantum dots have low yield and are difficult to control size distribution. The bottom-up method mainly uses various organic matters as carbon sources, carbonizes the organic matters through heat treatment to obtain the carbon quantum dots, and comprises the methods of hydrothermal synthesis, pyrolysis and the like, the methods can control the appearance and the size distribution of the carbon quantum dots, and the carbon quantum dots can be subjected to surface modification and passivation treatment through a modifier, so that the fluorescence characteristics and the electrical properties of the carbon quantum dots are improved. While optimizing the preparation scheme of the carbon quantum dots, people also find a new carbon source which can obtain high-yield fluorescent carbon quantum dots and is environment-friendly, for example, biomass such as straw, leaves, fruit peels, bagasse and the like is used as a carbon source, or waste is utilized, and industrial wastewater is used as the carbon source.
Tobacco is a plant belonging to the genus Nicotiana of the family Solanaceae, and more than 3000 compounds have been identified. The tobacco stem is the rough stem vein of the tobacco leaf and accounts for 1/3 of the weight of the tobacco leaf. The tobacco stem has the same components as tobacco leaf, and mainly comprises cellulose, lignin, pentosan, nicotine, pectin, tobacco leaf protein, solanesol, xylose and other organic substances, and also contains nitrogen, potassium, chlorine, sulfur and other elements. Tobacco enterprises can generate considerable tobacco waste water in the cigarette production process. According to statistics, the annual wastewater discharge of most tobacco processing enterprises in China reaches 175-600 km3. In the cigarette production process, the tobacco stem is cleaned by water, the humidity of tobacco shreds is adjusted, and the tobacco shreds are dried and moistened by steam in the tobacco shred making process, so that considerable tobacco waste water is generated. The tobacco waste water contains a large amount of fine suspended matters and woodThe organic substances such as lignin, nicotine, solanesol, carbohydrate, aromatic substances and the like, wherein the relative content of lignin, cellulose and carbohydrate is high. According to tests, the Chemical Oxygen Demand (COD) of the tobacco wastewater reaches 11000-13000 mg/L, the temperature of the wastewater is 45-70 ℃, a large amount of heat is contained, and if the wastewater is directly discharged without treatment, not only resource and energy waste is caused, but also serious environmental pollution is caused. In addition, because the substance structure contained in the tobacco wastewater is stable and complex, the anaerobic biochemical treatment of the tobacco wastewater by using the common industrial wastewater becomes a difficult problem, and the tobacco wastewater not only reaches the standard and is difficult to discharge, but also reaches the standard of regenerated reuse water.
Disclosure of Invention
Aiming at the problems in the tobacco wastewater treatment in the prior art, the invention provides a method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater, namely, the tobacco wastewater is used as a carbon source, the carbon quantum dots are prepared by simple pyrolysis reaction, and ethanol, deionized water, oxalic acid and sodium hydroxide solution are respectively used as modifiers to adjust the fluorescence wavelength of the carbon quantum dots so as to meet the actual application requirements.
The invention aims to utilize the tobacco wastewater as a resource, eliminate the hidden danger that organic matters in the tobacco wastewater pollute the environment from the source by adopting a simple manufacturing process, and simultaneously obtain a new carbon quantum dot material with high added value, thereby changing waste into valuable.
The invention has the advantages of simple process, low cost, energy and time conservation, easily obtained raw materials, rich resources, suitability for large-scale production, small investment, high return rate and quick response. Therefore, the invention can solve the problem of waste water treatment of the tobacco processing enterprises at present.
A method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater comprises the following specific steps:
(1) heating the tobacco wastewater to 200-300 ℃ at a constant speed, and heating and reacting for 1-3 h in the temperature range until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A;
(2) cooling the reaction product A in the step (1) to room temperature, adding a modifier into the reaction product A, and uniformly mixing to obtain a mixed solution B;
(3) and (3) stirring the mixed solution B obtained in the step (2) for 5-10 min, performing ultrasonic treatment for 5-10 min, standing, taking supernatant, performing centrifugal treatment, standing again, and taking supernatant to obtain the multicolor fluorescent carbon quantum dots dispersed in the modifier.
The modifier in the step (2) is ethanol, deionized water, oxalic acid solution or sodium hydroxide solution.
The ethanol is analytically pure, the concentration of the oxalic acid solution is 1-8 g/L, and the concentration of the sodium hydroxide solution is 1-8 g/L.
The volume ratio of the modifying agent to the reaction product A in the step (2) is (5-10): 1.
The rotating speed of the centrifugal treatment in the step (3) is 8000-12000 r/min, and the centrifugal time is 10-30 min.
The invention has the beneficial effects that:
(1) according to the invention, tobacco wastewater is used as a precursor, carbon quantum dots are prepared through a simple pyrolysis reaction, and ethanol, deionized water, oxalic acid or sodium hydroxide solution is respectively adopted as a modifier to disperse the carbon quantum dots, so that the fluorescence emission wavelength of the carbon quantum dots can be regulated and controlled;
(2) according to the invention, the carbon quantum dots are prepared by pyrolyzing the tobacco wastewater, the whole process from the raw material preparation process to the product is energy-saving and environment-friendly, the tobacco wastewater can be recycled, zero pollution discharge is realized, and the sewage discharge pressure of tobacco enterprises is effectively reduced;
(3) the method selects the tobacco wastewater as the carbon source to pyrolyze and synthesize the carbon quantum dots, has the advantages of simple process, low cost, energy and time conservation, suitability for large-scale production, easily available raw materials, abundant resources, environmental protection and capability of achieving the purposes of energy conservation and emission reduction;
(4) according to the invention, the tobacco wastewater is used as a carbon source, the pyrolysis method is used for preparing the carbon quantum dots, the high-concentration organic matters in the tobacco wastewater can be effectively degraded, the waste is changed into valuable, the carbon quantum dot luminescent material with high added value is produced, and meanwhile, economic benefits, ecological benefits and social benefits are generated;
(5) the carbon quantum dots synthesized by pyrolysis have the advantages of high crystallinity, uniform size, high fluorescence quantum efficiency, and good water solubility, dispersibility and light stability. The carbon quantum dots have low toxicity, so that the carbon quantum dots can be used in the fields of cell marking, biological imaging, drug delivery, fluorescent probes, photocatalysis, photoluminescence, electroluminescence films, devices and the like.
Drawings
FIG. 1 is a TEM image of the surface topography (a) and lattice fringes (b) of the carbon quantum dots and their corresponding Fourier transform (FFT) graph (inset in a) and particle size distribution graph (c) of example 1;
FIG. 2 is an X-ray photoelectron spectrum of the carbon quantum dots of example 1;
FIG. 3 is a high resolution scanning spectrum of the carbon quantum dot C1 s of example 1;
FIG. 4 is a high resolution scanning spectrum of the carbon quantum dot N1 s of example 1;
FIG. 5 is a high resolution scanning spectrum of the carbon quantum dot S2 p in example 1;
FIG. 6 is a graph comparing the absorption spectra (UV-Vis) of the carbon quantum dots of examples 1-4;
FIG. 7 shows the fluorescence spectrum of carbon quantum dots in example 1;
FIG. 8 is the fluorescence spectrum of the carbon quantum dots of example 2;
FIG. 9 is the fluorescence spectrum of the carbon quantum dots of example 3;
FIG. 10 is the fluorescence spectrum of the carbon quantum dots of example 4;
FIG. 11 is a graph comparing the strongest emission wavelengths and peak positions of the carbon quantum dots of examples 1-4;
FIG. 12 is a chromaticity diagram of the carbon quantum dots synthesized in examples 1 to 4.
Detailed Description
The invention will be further illustrated with reference to specific examples, without however restricting the scope of the invention thereto.
Example 1
A method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater comprises the following specific steps:
(1) putting 300 mL of tobacco wastewater in a beaker, placing the beaker on a heating platform, heating the beaker to 300 ℃ at a constant speed, and heating and reacting the beaker at the constant temperature of 300 ℃ for 3 hours until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A;
(2) after the reaction product A in the step (1) is cooled to room temperature, adding a modifier ethanol into the reaction product A and uniformly mixing to obtain a mixed solution B;
(3) magnetically stirring the mixed solution B obtained in the step (2) for 10 min, performing ultrasonic treatment for 5 min, standing, taking supernatant, performing centrifugal treatment, standing again, and taking supernatant to obtain blue fluorescent carbon quantum dots dispersed in ethanol; wherein the rotation speed of the centrifugal treatment is 12000r/min, and the centrifugal time is 30 min; the volume ratio of the modifying agent ethanol to the reaction product C is 10: 1;
in this embodiment, the surface topography of the carbon quantum dot is shown in fig. 1(a), the TEM image of the lattice fringes is shown in fig. 1(b) and the corresponding fourier transform (FFT) image is shown in the inset diagram in fig. 1(a), and as can be seen from fig. 1(a) to (b), the carbon quantum dot has good dispersibility and crystallinity, the lattice fringes are clear, and the spacing between crystal planes is 0.218 nm and corresponds to the graphene (1120) plane; the particle size distribution diagram of the carbon quantum dots is shown in FIG. 1(c), and it can be seen from FIG. 1(c) that the size distribution of the carbon quantum dots is 2 to 8 nm, and the average particle size is 4.90 nm;
the full spectrum of the carbon quantum dot X-ray photoelectron spectroscopy (XPS) of this example is shown in FIG. 2. from FIG. 2, it can be seen that the three peaks at 284.8 eV, 400.5 eV and 532.8 eV belong to the carbon core sp2Three peaks of C1S, N1S and O1S of the region at 378.0 eV, 285.98 eV and 168.86 eV belong to K2S, Cl 2p and S2 p respectively, and analysis shows that the atomic percentages of carbon, oxygen and nitrogen of surface constituent elements of the carbon quantum dots are 52.11%, 39.30% and 3.44% respectively, and the atomic percentages of potassium, chlorine and sulfur are 2.85%, 1.03% and 1.37% respectively;
the high resolution scanning spectrum of the carbon quantum dot C1S in the embodiment is shown in FIG. 3, the high resolution scanning spectrum of the carbon quantum dot N1S in the embodiment is shown in FIG. 4, the high resolution scanning spectrum of the carbon quantum dot S2 p in the embodiment is shown in FIG. 5, and as can be seen from FIGS. 3 to 5, the peak positions of the high resolution scanning spectrum C1S at 284.8 eV, 286.8 eV and 288.1 eV correspond to the binding energies of the C-C/C = C bond, C-O and O-C = O group, respectively; the peak positions of the high-resolution scanning spectrum N1 s at 399.8 eV and 401.5 eV respectively correspond to the binding energy of Pyridinic N and Graphitic N; the peak positions of the high resolution scan S2 p at 168.2 eV and 169.75 eV correspond to the bond energies of S-C-S and C-SOx, respectively.
Example 2
On the basis of the embodiment 1, the modifying agent is replaced by deionized water, and other conditions are not changed; the green fluorescent carbon quantum dots dispersed in the deionized water can be obtained.
Example 3
On the basis of the embodiment 1, the modifying agent is replaced by oxalic acid solution, the concentration of the oxalic acid solution is 1.8 g/L, and other conditions are not changed; yellow fluorescent carbon quantum dots dispersed in the oxalic acid solution can be obtained.
Example 4
On the basis of the example 1, the modifying agent is replaced by sodium hydroxide solution, the concentration of the sodium hydroxide solution is 1.8 g/L, and other conditions are unchanged; yellow fluorescent carbon quantum dots dispersed in sodium hydroxide solution can be obtained.
The ultraviolet-visible absorption spectra (UV-Vis) of the carbon quantum dots of examples 1-4 are shown in FIG. 6, wherein the absorption peaks of the ultraviolet-visible absorption spectra of the carbon quantum dots are all concentrated in the ultraviolet region of 200-400 nm; the fluorescence spectrum (PL) of the carbon quantum dots in example 1 is shown in FIG. 7, the fluorescence spectrum (PL) of the carbon quantum dots in example 2 is shown in FIG. 8, and the fluorescence spectrum (PL) of the carbon quantum dots in example 3 is shown in FIG. 9; example 4 the fluorescence spectrum (PL) of carbon quantum dots is shown in FIG. 10; as can be seen from FIGS. 8 to 10, the fluorescence spectra are all centered on the visible light band of 400 to 750 nm, and belong to typical photoluminescence fluorescent carbon quantum dots. As can be seen from fig. 11, under the same test conditions, the four carbon quantum dots dispersed in different modifiers (ethanol, deionized water, oxalic acid solution and sodium hydroxide solution) respectively exhibit the strongest fluorescence emission under the excitation of monochromatic light with wavelengths of 380 nm, 460 nm, 470 nm and 470 nm, and the corresponding emission wavelengths are 462 nm, 548 nm, 563 nm and 565 nm. Compared with the carbon quantum dots prepared in the embodiments 2 to 4, the carbon quantum dots dispersed in the ethanol solution prepared in the embodiment 1 have stronger absorption and strongest fluorescence. The carbon quantum dots prepared by the tobacco wastewater can be subjected to surface modification by the modifier, so that the fluorescence wavelength of the carbon quantum dots can be regulated and controlled, and the fluorescence intensity of the carbon quantum dots can be enhanced.
The chromaticity diagram of the carbon quantum dots of examples 1-4 is shown in FIG. 12, wherein numerals 1-4 represent the positions of the carbon quantum dots prepared in examples 1-4 on the chromaticity diagram respectively; as can be seen from FIG. 12, the carbon quantum dots prepared by the present invention have good fluorescence properties, and the fluorescence wavelength can be adjusted from a blue region to a yellow region. The fluorescence quantum yield can reach and exceed 16% through measurement and calculation.
Example 5
A method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater comprises the following specific steps:
(1) putting 200 mL of tobacco wastewater in a beaker, placing the beaker on a heating platform, heating the beaker to 260 ℃ at a constant speed, and heating and reacting the beaker at the constant temperature of 260 ℃ for 2 hours until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A;
(2) after the reaction product A in the step (1) is cooled to room temperature, adding a modifier ethanol into the reaction product A and uniformly mixing to obtain a mixed solution B;
(3) magnetically stirring the mixed solution B obtained in the step (2) for 5 min, performing ultrasonic treatment for 10 min, standing, taking supernatant, performing centrifugal treatment, standing again, and taking supernatant to obtain blue fluorescent carbon quantum dots dispersed in ethanol; wherein the rotation speed of the centrifugal treatment is 10000 r/min, and the centrifugal time is 10 min; the volume ratio of the modifying agent ethanol to the reaction product C is 8: 1.
Example 6
On the basis of the embodiment 5, the modifying agent is replaced by deionized water, and other conditions are not changed; the green fluorescent carbon quantum dots dispersed in the deionized water can be obtained.
Example 7
On the basis of the embodiment 5, the modifying agent is replaced by oxalic acid solution, the concentration of the oxalic acid solution is 7.2 g/L, and other conditions are not changed; yellow fluorescent carbon quantum dots dispersed in the oxalic acid solution can be obtained.
Example 8
On the basis of the embodiment 5, the modifying agent is replaced by sodium hydroxide solution, the concentration of the sodium hydroxide solution is 7.2 g/L, and other conditions are not changed; yellow fluorescent carbon quantum dots dispersed in sodium hydroxide solution can be obtained.
Example 9
A method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater comprises the following specific steps:
(1) putting 100 mL of tobacco wastewater in a beaker, placing the beaker on a heating platform, heating the beaker at a constant speed until the temperature is 200 ℃, and heating the beaker at the constant temperature of 200 ℃ for 1 hour until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A;
(2) after the reaction product A in the step (1) is cooled to room temperature, adding a modifier ethanol into the reaction product A and uniformly mixing to obtain a mixed solution B;
(3) magnetically stirring the mixed solution B obtained in the step (2) for 6 min, performing ultrasonic treatment for 8 min, standing, centrifuging the supernatant, standing again, and taking the supernatant to obtain blue fluorescent carbon quantum dots dispersed in ethanol; wherein the rotation speed of the centrifugal treatment is 8000 r/min, and the centrifugal time is 20 min; the volume ratio of the modifying agent ethanol to the reaction product C is 5: 1.
Example 10
On the basis of the example 9, the modifier is replaced by deionized water, and other conditions are not changed; so as to obtain the green fluorescent carbon quantum dots dispersed in the deionized water.
Example 11
On the basis of the embodiment 9, the modifying agent is replaced by oxalic acid solution, the concentration of the oxalic acid solution is 5.6 g/L, and other conditions are not changed; yellow fluorescent carbon quantum dots dispersed in the oxalic acid solution can be obtained.
Example 12
On the basis of example 9, the modifier is replaced by sodium hydroxide solution, the concentration of the sodium hydroxide solution is 5.6 g/L, and other conditions are unchanged; yellow fluorescent carbon quantum dots dispersed in the sodium hydroxide solution can be obtained;
table 1 shows a comparison table of preparation process parameters of carbon quantum dots of examples 1-12;
as can be seen from Table 1, the emission wavelength of the fluorescent carbon quantum dots can be adjusted from a blue region to a yellow region by respectively using ethanol, deionized water, oxalic acid and sodium hydroxide solution as modifiers.
Claims (3)
1. A method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater is characterized by comprising the following specific steps:
(1) heating the tobacco wastewater to 200-300 ℃ at a constant speed, and heating and reacting for 1-3 h in the temperature range until organic matters are dehydrated, carbonized and discolored to obtain a reaction product A;
(2) cooling the reaction product A in the step (1) to room temperature, adding a modifier into the reaction product A, and uniformly mixing to obtain a mixed solution B; wherein the modifier is ethanol, deionized water, an oxalic acid solution or a sodium hydroxide solution, the ethanol is analytically pure, the concentration of the oxalic acid solution is 1-8 g/L, and the concentration of the sodium hydroxide solution is 1-8 g/L;
(3) and (3) stirring the mixed solution B obtained in the step (2) for 5-10 min, carrying out ultrasonic treatment for 5-10 min, standing, taking supernatant for centrifugal treatment, standing again, and taking supernatant to obtain the multicolor fluorescent carbon quantum dots dispersed in the modifier.
2. The method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater as claimed in claim 1, wherein the method comprises the following steps: the volume ratio of the modifier to the reaction product A in the step (2) is (5-10): 1.
3. The method for preparing multicolor fluorescent carbon quantum dots by using tobacco wastewater according to claim 1, wherein the method comprises the following steps: the rotating speed of the centrifugal treatment in the step (3) is 8000-12000 r/min, and the centrifugal time is 10-30 min.
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| CN110511751B (en) * | 2019-08-28 | 2022-04-19 | 西南大学 | Tunable dual-emission fluorescent carbon dot, and preparation method and application thereof |
| CN110451483B (en) * | 2019-09-02 | 2021-10-29 | 中国农业科学院郑州果树研究所 | Preparation method for synthesizing fluorescent carbon quantum dots by taking kiwi fruits as raw materials |
| CN113148979B (en) * | 2021-02-05 | 2022-11-08 | 贵州省烟草科学研究院 | Method for preparing carbon dots with different colors under same wavelength by using tobacco waste and application |
| CN114852992A (en) * | 2022-02-09 | 2022-08-05 | 云南大学 | Method for separating and extracting carbon dots from smoke dust wastewater of thermal power plant |
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